Sm2O3/ZnO nanoparticles were prepared via microwave-assisted hydrothermal and sol-gel combustion synthesis. Characteristics of obtained samples were compared in dependence of Sm2O3 content and calcination temperature. Prepared nanostructures were characterized with scanning electron microscopy and X-ray diffraction. Nanoparticles prepared via microwave-assisted hydrothermal and sol-gel method have flower-like and spherical shape respectively. The photocatalytic activity of samples under solar light simulated illumination was found to be affected by content of Sm2O3, calcination temperature and preparation method. The first-order rate constant of MB solution degradation of samples prepared via microwave-assisted hydrothermal method approximately three times exceeds that of sol-gel samples.